Open AccessSealing Effect of Magic-Angle-Spinning Rotors in Solid-State NMR
Author(s) -
Shigenobu Hayashi
Publication year - 2009
Publication title -
analytical sciences
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.392
H-Index - 73
eISSN - 1348-2246
pISSN - 0910-6340
DOI - 10.2116/analsci.25.133
Subject(s) - chemistry , magic angle spinning , solid state nuclear magnetic resonance , anhydrous , nmr spectra database , spinning , magic angle , spectral line , nuclear magnetic resonance spectroscopy , analytical chemistry (journal) , solid state , nuclear magnetic resonance , chromatography , organic chemistry , polymer chemistry , physics , astronomy
Several methods are proposed to check the sealing of a magic-angle-spinning (MAS) rotor. The intrusion of moisture into the MAS rotor is checked by trimethylphosphine oxide, which is highly hygroscopic. Its hydrated form is separately observed in (31)P MAS NMR spectra from the crystalline (anhydrous) form. (1)H MAS NMR can monitor the hydrated form, the crystalline form, and adsorbed water independently. Gas leakage from the MAS rotor is monitored by measuring (129)Xe MAS NMR spectra of xenon (Xe) confined in zeolites as well as (3)He MAS NMR spectra of (3)He gas. The sealing effect of MAS rotors has been checked quantitatively using the above methods.